Substitution of Cupric Sulfate for Mercuric Oxide as Catalyst for the Kjel-Foss Instrument

1976 ◽  
Vol 59 (1) ◽  
pp. 219-220
Author(s):  
Larry L Wall ◽  
Charles W Gehrke
Keyword(s):  
Standard Deviation ◽  
Mercuric Oxide ◽  
Experimental Sample ◽  
Cupric Sulfate ◽  
Protein Nitrogen ◽  
Feed Control ◽  
Relative Standard ◽  
Standard Configuration ◽  
Automated Instrument

Abstract A mixture of cupric sulfate and titanium dioxide and cupric sulfate alone were evaluated as possible catalysts to replace mercuric oxide in the determination of protein nitrogen, using the Kjel-Foss automated instrument. It was necessary to modify the instrument to increase the digestion time from 6 to about 12 min to achieve acceptable protein nitrogen recovery with cupric sulfate as the catalyst. An experimental sample set of nitrogen-containing salts and American Association of Feed Control Officials check feed samples were analyzed with the Kjel-Foss instrument in its standard configuration with mercuric oxide and as modified with cupric sulfate as the catalyst. The average per cent nitrogen, standard deviation, and relative standard deviation with mercuric oxide and cupric sulfate were 10.37 and 10.36, 0.040 and 0.042, and 0.53 and 0.56, respectively. The substitution of cupric sulfate for mercuric oxide is feasible, and it eliminates the use of the potential pollutant, mercury.

Microcomputer Controlled Titration for Determination of Protein Nitrogen in Feeds and Wheat

1979 ◽  
Vol 62 (5) ◽  
pp. 969-975
Author(s):  
Alan H B Wu ◽  
Taddeo Rotunno ◽  
Howard V Malmstadt
Keyword(s):  
Standard Deviation ◽  
Copper Catalysts ◽  
Protein Nitrogen ◽  
Sample Number ◽  
Testing Program ◽  
Direct Titration ◽  
Relative Standard ◽  
Automatic Titrator ◽  
Feed Samples

Abstract The determination of protein nitrogen in feeds and wheat by microcomputer controlled titration is described. The method involves direct titration of ammonia with standard hypochlorite titrant in the presence of bromide. The titrant is delivered by an automatic buret, and the microcomputer controlled, automatically computed potentiometric end points are precise to 0.1% over a 5-fold concentration range of nitrogen. Digestions performed with both mercury and copper catalysts show comparable results. Samples are weighed before digestion by an electronic balance interfaced to the computer which records sample number and weight. An automatic pipet aliquots, dilutes, and buffers samples directly from the digestion tubes; the samples can be immediately titrated with the automatic titrator. The results for protein in NBS standards and check feed samples from an official testing program compare closely with average values reported for these standards. Results show that feed and wheat samples contained 10- 100% protein. Precision for successive aliquots of the same digests is 0.1-0.4% relative standard deviation; precision for multiple digestions of the same sample is 0.1-0.8%.

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.

Determination of Nitrate in Water by HPLC

2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Recovery Rate ◽  
High Performance ◽  
Separation Efficiency ◽  
Fast Analysis ◽  
Relative Standard

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%～105.7%,the relative standard deviation（RSD）wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).

scholarly journals Determination of Sodium Cromoglycate by a New Kinetic Spectrophotometric Method in Biological Samples

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Mohsen Keyvanfard ◽  
Khadijeh Alizad ◽  
Razieh Shakeri
Keyword(s):  
Standard Deviation ◽  
Sodium Cromoglycate ◽  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Biological Samples ◽  
Limit Of Detection ◽  
Micellar Medium ◽  
Relative Standard ◽  
Kinetic Spectrophotometric

A new kinetic spectrophotometric method is described for the determination of ultratrace amounts of sodium cromoglycate (SCG). The method based on catalytic action of SCG on the oxidation of amaranth with periodate in acidic and micellar medium. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of the amaranth at 518 nm, for the first 4 min from initiation of the reaction. Calibration curve was linear in the range of 4.0−36.0 ng mL−1SCG. The limit of detection is 2.7 ng mL−1SCG. The relative standard deviation (RSD) for ten replicate analyses of 12, 20, and 28 ng mL−1SCG was 0.40%, 0.32%, and 0.53%, respectively. The proposed method was used for the determination of SCG in biological samples.

scholarly journals Determination of 1,3-Dichloropropanol in Soy Sauce and Related Products by Headspace Gas Chromatography with Mass Spectrometric Detection: Interlaboratory Study

2005 ◽  
Vol 88 (5) ◽  
pp. 1404-1412 ◽  
Author(s):  
Sarah Hasnip ◽  
Colin Crews ◽  
Nicholas Potter ◽  
Paul Brereton ◽  
Henri Diserens ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Internal Standard ◽  
Mass Spectrometric ◽  
Soy Sauce ◽  
Headspace Gas Chromatography ◽  
Relative Standard ◽  
Headspace Gas

Abstract An interlaboratory study was performed to evaluate the effectiveness of a headspace gas chromatography (GC) method for the determination of 1,3-dichloro-propan-2-ol (1,3-DCP) in soy sauce and related products at levels above 5 ng/g. The test portion is mixed with an internal standard (d5-1,3-DCP) and ammonium sulfate in a sealed headspace vial. After achieving equilibrium, the headspace is sampled either by gas-tight syringe or solid-phase microextraction (SPME) and analyzed by GC with mass spectrometric detection. 1,3-DCP is detected in the selected-ion mode (monitoring m/z 79 and 81 for 1,3-DCP and m/z 82 for the deuterated internal standard) and quantified by measurement against standards. Test materials comprising soy, dark soy, mushroom soy, and teriyaki sauces, both spiked and naturally contaminated, were sent to 9 laboratories in Europe, Japan, and the United States; of these, 5 used SPME and 4 used syringe headspace analysis. Test portions were spiked at 5.0, 10.0, 20.0, 100.0, and 500.0 ng/g. The average recovery for spiked blank samples was 108% (ranging from 96–130%). Based on results for spiked samples (blind pairs at 5, 10, 20, 100, and 500 ng/g) as well as a naturally contaminated sample (split-level pair at 27 and 29 ng/g), the relative standard deviation for repeatability (RSDr) ranged from 2.9–23.2%. The relative standard deviation for reproducibility (RSDR) ranged from 20.9–35.3%, and HorRat values of between 1.0 and 1.6 were obtained.

scholarly journals Spectrophotometric flow injection procedure to indirect determination of paracetamol in pharmaceutical formulations using o-tolidine as reagent

2018 ◽  
Vol 33 (2) ◽  
pp. 47
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira
Keyword(s):  
Standard Deviation ◽  
Detection Limit ◽  
Flow Injection ◽  
Pharmaceutical Formulations ◽  
Injection Method ◽  
Indirect Determination ◽  
Analytical Curve ◽  
Relative Standard ◽  
Injection Procedure

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.

scholarly journals A kinetic method for the determination of phenol

2002 ◽  
Vol 67 (10) ◽  
pp. 661-667 ◽  
Author(s):  
Snezana Mitic ◽  
Valentina Zivanovic
Keyword(s):  
Standard Deviation ◽  
River Water ◽  
Reaction Rate ◽  
Kinetic Method ◽  
Potassium Periodate ◽  
Experimental Conditions ◽  
Inhibiting Effect ◽  
Relative Standard ◽  
Kinetic Expression

Akinetic method for the determination of phenol is proposed. The method is based on the inhibiting effect of phenol on the Mn(II) catalysis of the oxidation of malachite green with potassium periodate. The reaction rate was followed spectrophotometrically at 615 nm. Kinetic expression for the reaction in the presence and absence of phenol are postulated. The optimal experimental conditions for the determination of phenol were established and phenol was determined in concentrations from 30.0 to 188.0 ng/cm3 with a relative standard deviation of 5.5%. The lower detecton limit is 7.8 ng/cm3. The effects of certain foreign ions upon the reaction rate were determined for the assessment of the selectivity of the method. The method was applied for the determination of phenol in tap and river water.

scholarly journals Development and validation of spectrophotometric method for phenylephrine hydrochloride estimation in nasal drops formulations

2008 ◽  
Vol 27 (2) ◽  
pp. 149 ◽  
Author(s):  
Ivana Savić ◽  
Goran Nikolić ◽  
Vladimir Banković
Keyword(s):  
Standard Deviation ◽  
Sodium Hydroxide ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Development And Validation

Simple, accurate and reproducible UV-spectrophotometric method was developed and validated for the estimation of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. Phenylephrine hydrochloride was estimated at 291 nm in 1 mol⋅dm-3 sodium hydroxide (pH 13.5). Beer’s law was obeyed in the concentration range of 10–100 μg⋅cm−3 (r2 = 0.9990) in the sodium hydroxide medium. The apparent molar absorptivity was found to be 1.63×103 dm3⋅mol−1⋅cm−1. The method was tested and validated for various parameters according to the ICH (International Conference on Harmonization) guidelines. The detection and quantitation limits were found to be 0.892 and 2.969 μg⋅cm−3, respectively. The proposed method was successfully applied for the determination of phenylephrine hydrochloride in pharmaceutical nasal drops formulations. The results demonstrated that the procedure is accurate, precise and reproducible (relative standard deviation < 1 %), while being simple, cheap and less time consuming, and hence can be suitably applied for the estimation of phenylephrine hydrochloride in different dosage forms.

scholarly journals Badanie stabilności barwnych znaczników fluorescencyjnych w silnie zasiarczonych wodach złożowych

Nafta-Gaz ◽  
2021 ◽  
Vol 77 (2) ◽  
pp. 82-91
Author(s):  
Katarzyna Wojtowicz ◽  
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Rhodamine B ◽  
Water Reservoir ◽  
Distilled Water ◽  
Test Results ◽  
Fluorescent Tracers ◽  
Reservoir Water ◽  
Relative Standard

The article presents the issues related to the determination of colored fluorescent tracers such as fluorescein, eosin yellowish, rhodamine B and uranine in reservoir waters by spectrophotometric method. For this purpose, the influence of the pH of the solution on the absorption spectra of the tested tracers was checked. Test results show that fluorescein, rhodamine B and uranine are sensitive to changes in the buffer pH, therefore it is advisable to use stable tracer solutions as well as to control and possibly correct pH in further tests. As part of the study, calibration curves of fluorescein, eosin yellowish, rhodamine B and uranine in distilled water, reservoir water A4 and highly sulfated reservoir waters A5 and A6 were plotted and the analytical methods were validated. Analytical validation included determination of linearity, standard deviation and relative standard deviation of the tested tracers solutions. High values of the regression parameters (0.9927–0.9998) of the analyzed tracers prove a good linear fit, while low values of standard deviation and relative standard deviation prove its repeatability and precision. Particular attention was paid to testing the stability of colored fluorescent tracers in highly sulfated reservoir waters. For this purpose, solutions of the tested tracers were prepared at concentrations of 10 mg/dm3 in distilled water, A4 reservoir water and highly sulfated A5 and A6 reservoir waters. Measurements of the tested tracers in the prepared solutions were performed every 2 days over the period of 1 month. The test results show that fluorescein, eosin yellowish, rhodamine B and uranine solutions are stable in the distilled water and A4 reservoir water, while they degrade in the A5 and A6 reservoir waters. Fluorescein and uranine turned out to be the most sensitive, as they degraded completely in the A6 reservoir water after 20 (fluorescein) and 22 (uranine) days. Yellowish eosin and rhodamine B turned out to be slightly more stable in highly sulfated reservoir waters, as they degraded completely in the A6 reservoir water after 24 days.

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